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Author: Subject: Series of ETN nitration problems
underground
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[*] posted on 4-6-2018 at 06:12


Ok today i tried another small batch as i described above but this time i increase the temp to 35 C at the last 30 min. I did not got any yields. It looks like the safe temp, at least with this method, is somewhere between 20-35 C. I really have no idea how patents go up to some crazy temps like 40-60 C. I won't never again try to go above 20 C, i believe it doesnt worth. Next time i will try to scale it up to 200ml SA and see how it will work.
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XeonTheMGPony
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[*] posted on 4-6-2018 at 19:17


you really need to distill the acid, I had superior results with care fully distilled H2SO4. this eliminates a huge variable!
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Laboratory of Liptakov
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[*] posted on 4-6-2018 at 21:17


I have same opinion as Xeon. Undeground, You need distillation assembly. For SA and for NA. And for 100 next procedures. Both are basic compound of all researcher. Testing different temperatures are the blind way. In this problem of low yields.



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XeonTheMGPony
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[*] posted on 6-6-2018 at 04:14


Yup just no getting around some basic core glass wear, where not having it is actually dangerous to you and others.

I even care fully distill my acetone even for use as a solvent and I have found large amounts of crap after wards at time.

You need to remove variables and drain cleaner sulfuric is a big one.

Next what was the original source of the Erythritol? If pure it will be good.
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[*] posted on 6-6-2018 at 05:16


I can see your points Laboratory and Xeon but i really want to keep things as much simple as possible. Anyway i did another nitratation and the yields really shocked me, maybe i got close to 80-90%, they are still drying, i can tell you precisely after it will be completely dry. I used 400gr H2SO4 (about 219ml 98%), 120gr Kno3, 21g E (I should have use 30g but i reduced the ammount to 21g thinking that i could reduce the lower nitrated esters and looks like it worked). The procedure was exactly as Laboratory said to me. Yields looking close to 40g recrystalized. :D

[Edited on 6-6-2018 by underground]
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roXefeller
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[*] posted on 6-6-2018 at 18:22


Quote: Originally posted by underground  
I can see your points Laboratory and Xeon but i really want to keep things as much simple as possible.


If you want simple, go with acetone peroxide. Explosives aren't something we enter into looking for the simplest routes. You wouldn't jump out of an airplane with a kite just because it was easy to buy and parachutes were sold out. Get the tools, glassware, and the reagents that are necessary before jumping out the door. ETN was the very compound that started the "Life after detonation" thread.

And why are you scaling up your reaction when you're still working out the parameters?
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[*] posted on 7-6-2018 at 12:01


Quote: Originally posted by roXefeller  

If you want simple, go with acetone peroxide. Explosives aren't something we enter into looking for the simplest routes. You wouldn't jump out of an airplane with a kite just because it was easy to buy and parachutes were sold out. Get the tools, glassware, and the reagents that are necessary before jumping out the door. ETN was the very compound that started the "Life after detonation" thread.

And why are you scaling up your reaction when you're still working out the parameters?


Actually, the place where I am working does not have electricity and i cant bring electricity there too. Even if i bought the equipment i could not work with it.

Now i am scaling my reactions up cause yields are very good already and i did not have much ETN left over. Also i have plenty of reagents so I don't mind to scale it up a bit.
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[*] posted on 8-6-2018 at 06:52


Haha....Parachutes were sold out... But : Explosives aren't something we enter into looking for the simplest routes. Truth,. Next: High yields?
Erythritol were dissolved in H2SO4 ? Works it ? Low temperature were used ? I am glad to hear it.....:-)....:cool:




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